反应详情

温度

55 °C

A mixture of 3-aminobenzamide (68 mg, 0.5 mmol), 9B (92 mg, 0.5 mmol) and glyoxylic acid monohydrate (46 mg, 0.5 mmol) in acetonitrile (3.0 mL) and DMF (0.8 mL) was heated at 55° C. for 18 h. After removal of solvent, the crude was purified by silica gel column chromatography eluting with gradient methanol in methylene chloride to give 9C as a solid (100 mg, 60% yield). 1H NMR (400 MHz, Methanol-d4) δ ppm 1.25 (t, J=6.81 Hz, 3H) 3.96 (m, 2H) 5.03 (s, 1H) 6.70 (d, J=7.91 Hz, 1H) 6.96-7.08 (m, 5H) 7.15 (dd, J=8.35, 1.76 Hz, 1H); LC-MS 333 (M+H).

1. customAfter removal of solvent
2. customthe crude was purified by silica gel column chromatography
3. washeluting with gradient methanol in methylene chloride